Treatment of sugar solutions



Oct. 27, 1942. M. R ALLEN TREATMENT oF SUGAR SOLUTIONS Filed May s1, 1940 2 Sheets-Sheet 1 Oct 27 1942- M. R. ALLEN 2,299,783 TREATMENT 0F SUGAR soLuToNs Filed May s1, 1940 2 sheets-Sheet 2 INVENTOR Marg/1 azzzzen the line af-a,

Patented ct. 27, 1942` wam 'rasa'rmnn'r or sucka summons mnhdlnmie'arinmay,omo- Application my 31,1940, seem Ne. 338,105

1 claims` (cl. 12v-c1) This invention relates generally to the treatment of sugar solutions and more particularly to the treatment of such solutions containing alkaline earth metal salts to inhibit the formation of scale on. surfaces in contact with said solutions during evaporation. l

In the accompanying drawings, which illustrate a preferred embodiment of my invention:

Figs. 1 and 1a. taken together and Joined along constitute a flow sheet whichlllustrates in a diagrammatic manner one way of carrying out my process; and

Fig. 2 is a diagrammatic illustration of a quad-l ruple eifect evaporator usedA in concentrating thev sugar solution. y

When the liquor or solution obtained by soaking the sugar beets or the juice expressed from sugar cane is evaporated following defecation, considerable difficulty is always experienced due to the formation of scale on the heat transfer surfaces of the evaporators. This scale usually consists predominantly of calcium sulphate but may contain' calcium oxalate, calcium sulphite, calcium carbonate or the corresponding magnesium salts,

as well as various organic compounds. The sugar solution contains considerable' amounts of calcium and magnesium salts derived from the sugar beets or from the sugar cane. In addition. it is common practice inthe defecation or purification of the juices to add lime, in order to coagulate various albuminous materials. A certain proportion of the lime salts thus formed are car- -riedthrough the process and cause trouble, due to scale formation on the surfaces of the evaporator with which the solution contacts. It is an object of the present invention to inhibit the deposition of salts of calcium and the other alkaline earth metals, aswell as salts of' magnesium.

Previous attempts have been made to decrease the formation of scale in the evaporators by adding various materials in the defecation process. One of these has involved the addition of orthoquired for taking we of the nesium. In these eases, it was necessary to add an. amount of phosphoric acid or soda ash which was stoichiometricaliy suiiicient for causing the precipitation of the calcium and magnesium.

This necessarilyv involved the addition of large quantities of these materials and made the proc- `phosphoric acid or its salts to the thin Juice in an attempt to precipitate al1 the calcium in the form of calcium phosphate before the juice enters the evaporators.- Another method consists in adding `soda ash between the different stages of evaporation in an attempt to precipitate the calcium salts as. carbonate with the expectation that this would result in somewhat less scale formation than would be the case vif the calcium sulphate was allowed to deposit onthe surfaces. Neither of these-methods has proved entirely successful.

They'are both'open to the objection that relatively large amounts of added materials are esses quite expensive.

For the sake of brevity, I shall refer to calcium and its salts in the further description of the process. it being understood that magnesium and l its salts act similarly in their reactions with various materials and in their tendency to form scale during evaporation of the sugar solution. As contrasted with the relatively large amounts of reagents required to precipitate the calcium ac-l cording to prior methods, I have found thatl may prevent or materially decrease the amount of scale formed during evaporation of the juice by providing in the juice a relatively small amount of certain materials. I have found that this result may be accomplished by providing in the Juice a few parts per million based on the weight of the juice of a molecularly dehydrated alkali-metal phosphate. These phosphates are preferably added tothe sugar solution during or between stages of evaporation thereof but they may be added, as willbe explained'more fully hereinafter, to the condenser water used in condensing the steam from the last effect evaporator. This condenser water containing the molecularly dehydrated phosphate is then returned to the soaker for extractingjurther quantities'of sugar from the beetsv or'sugar cane to make further quantities of sugar solution, .which is then puriiied and evaporated. I preferto add molecularly creases the precipitation of calcium sulphate, call cium oxalate, calcium carbonate, calcium sulphite and other calcium salts which would otherwise form scale on the surfaces of the evaporator.

The preferred molecularly dehydrated alkalimetal phosphate is'the glassy water soluble metaphosphate commonly known as Grahams salt or sodium` hexametaphosphate. Sodium hexametaphosphate is a glassy material having a ratio of NaOto PzOt of 1:1. It will beundercalcium and magstood that sodium hexametaphosphate is given as representative of the family oi' glassy molecularly dehydrated alkali-metal phosphates and that other glassy molecularly dehydrated alkali-metal phosphates having a ratio of NazO to P205 between 0.9:l and 1.7:l, such as the so-called sodium tetraphosphate NasPIOis, with a ratio of NazO to P205 of 1.5:1, or the so-called sodium decaphosphate Na1aP1oO31,with a ratio of NazO to P205 of 1.2:1, may be used in place of or in addition to sodium hexametaphosphate. All of these glassy molecularly dehydrated alkali-metal phosphates have properties which are similar to one another, although differing somewhat in their effectiveness. In place of or in addition to the sodium hexametaphosphate or the other glassy molecularly dehydrated alkali-metal phosphates, I may use the alkali-metal tripolyphosphates-for example, sodium tripolyphosphates NasPaOio-or the alkali-metal pyrophosphatesfor example, tetra-sodium pyrophosphate Na4P2O1. I prefer, however, to use the glassy molecularly dehydrated alkali-metal phosphates and of these I perfer those members having properties substantially like sodium hexametaphosphate.

The term molecularly dehydrated alkali-metal phasphate is intended to include the metaphosphate, tripolyphosphate or pyrophosphate or mixtures of any of these phosphates. All of these molecularly dehydrated phosphates may be considered as derived from orthophosphates by the elimination of water of constitution. The molecularly dehydrated phosphates contain less water of constitution than the corresponding orthophosphates and have, therefore, come to be recognized as molecularly dehydrated phosphates, as pointed out more fully in the Hall and Jackson Patent 1,903,041, granted March 28, 1933.

Although the sodium salts are preferred, I may use the corresponding salts of the other alkalimetals, such as potassium or lithium.

Referring now more particularly to the accompanying drawings, the liquor obtained by soaking the beets in soaker I, or the juice expressed from sugar cane is ltered in filter 2 and is then purled or defecated in a defecator 3. Lime is added to the defecator in order to coagulate the albuminoids and sulphur dioxide or other'bleaching agent is added and the liquor is filtered in a filter 4. The filtered liquor is then evaporated, the evaporator illustrated in the drawings consisting of a quadruple effect evaporator having four effects 5, 6, 1 and 8. yThis evaporator is illustrated more in detail in Fig. 2. The sugar solution to be evaporated enters the first effect or vessel 5 through a pipe III. 'I'he vessel 5 is provided with an upper header I I and a lower header I2 through which pass tubes I3. Steam is led into the vessel through pipe I I into the space I5 which surrounds the tubes I3 between the tube headers. The sugar solution indicated by the numeral I6 passes through the tubes I 3 which are heated on their outside by the steam in compartment I5. The level of the sugar solution in the vessel 5 is indicated by the numeral I1. Each of the vessels or effects 6, 1 and 8 are similar in construction to the vessel 5 and need not be described in detail.

The steam entering vessel 5 through pipe I4 converts a certain amount of the water of the sugar solution into steam which passes through pipe I8 and is led into'the steam compartment I5a of vessel 6. In vessel 6, the solution is further concentrated a-nd the 'in is led through pipe I8d to steam compartment lib of the vessel 1. Similarly further concentration takes place in the vessel 1 and the steam issuing therefrom is passed through a pipe I8b to the steam compartment I5c of vessel 8. The steam coming from vessel 8 passes through a pipe 20 to a condenser 2| shown in Fig. la. This condenser maintains the vessels 8 and 1 under vacuum, the vacuum in vessel 8 being greater than that in vessel 1. The vessel 6 is kept at approximately atmospheric pressure, while vessel 5 is under a few pounds pressure. 'I'he arrangement is such that the decreased pressure on the sugar solution as it passes through the vessels 5, 6, 1 and 8 causes the evaporation in the dill'erent vessels by the steam led into each vessel from the preceding vessel.

The sugar solution passes between the vessels through the pipes 22, 22a and 22h and is discharged through pipe 22c to crystallizing pans where it precipitates as crystalline' sugar. The condensate from the steam ln compartments I5, I5a, I5b and I 5c passes through pipes 23, 23a, 23h and is discharged through pipe 23e.

Since very little scale ordinarly forms in the rst and second eiects or bodies of the evaporator, I usually add the sodium hexametaphosphate or other molecularly dehydrated alkalimetal phosphate to the sugar liquor between the second and third effects in the amount found necessary, usually between about 2 P. P. M. and 10 P. P. M., .based on the weight of the thin juice entering the first effect. When a quadruple effect evaporator is used, I have found it desirable to add an additional amount, usually between about 2 P. P. M. and 10 P. P. M. of the metaphosphate to the juice entering the fourth effect in addition to that added between the second and third eilects. This is in order to overcome the loss due to adsorption and reversion of the metaphosphate to orthophosphate.

In accordance with a modification of the above n described process, I may add the sodium hexametaphosphate or other molecularly dehydrated alkali-metal phosphate to the condenser water used in condensing the steam from the last effect evaporator. Thus, as shown in Fig. 1a, the cooling water which is supplied to the cooling coil 25 in the condenser 2| is fed into the coil through a pipe 26. This cooling Water may have added to it a few parts per million of molecularly dehydrated alkali-metal metaphosphate, for example 5 P. P. M. of sodium hexametaphosphate. The water passing through the cooling coil 25 condenses the steam entering the condenser through the pipe 20, thereby providing the vacuum in the evaporator vessels previously referred to. The water passing. through coil 25 is heated in the condenser and is then passed through pipe 21 to the soaker I for treating a further quantity of sugar: beets or sugar cane. The process then follows the cycle which has been previously described.

In some cases, it may be advisable to add a few parts per million of the molecularly dehydrated phosphate to the condenser water as well Steam Produced thereas to add a few parts per million of the molecularly dehydrated phosphate to the sugar solution between or during its stages of evaporation. In any event, the total of molecularly dehydrated alkali-metal phosphate which is-added is only a few parts per million and is much less than the stoichiometric amount in the sugar liquor.

which would be required to precipitate the calcium l Although I have illustrated and described one `phosphate between about '2 P. P. P. P. M. based on having a ratio of NazO 4 which comprises adding ners in which the process may be carried out, the

invention may be otherwise practiced within the scope of the following claims.

I claim:

1. In the treatment of sugar solutions containing alkaline earth metal salts, the process of inhibiting the formation of `scale on surfaces ln contact with said solution during evaporation, which comprises providing in said solution an amount of molecularlyv dehydrated alkali-metal the weight of the sugar solution entering the iirst effect evaporator.

2. In the treatment of sugar solutions `containing alkaline earth metal salts, the process of inhibiting the formation of scale on surfaces in.` contact with said lsolution during evaporation, which comprises adding to the sugar solution between stages of evaporation thereof molecularh1 dehydrated alkali-metal phosphate in amount between about/2 P. P. M. andlO P. P. M. based on the weight of the sugar solution entering the first eifect evaporator.

3. In the treatment of sugar solutions containing alkaline earth metal salts, the process of inhibiting the formation of scale on surfaces in contact with said solution duringevaporation, which comprises adding to the sugar solution between stages of evaporation thereof glassy molecularly dehydrated alkali-metal phosphate to P205 between 0.9;1 and 13:1, in amount between about 2 P. P. M. and P. P. M. based on the weight of the sugar solution entering the rst effect evaporator.

ing alkaline earth metal salts, the process of inhibiting `the formation of scale on surfaces in contact with vsaid solution during evaporation, to the condenser water used in condensing the steam from the evap- M. and 10/ an amount of, glassy `molecularlv dehydrated orator an amount of molecular-ly ,dehydrated alkali-metal phosphate between about 2 P. P. M. and 10 P. P. M. based on the weight of the condenser water, and utilizing the thus treated condenser water in extracting sugar to make sugar solution which is to be evaporated.

5. In the treatment of sugar solutions containing alkaline earth metal salts, the process of inhibiting the formation of scale on surfaces in contact 'with said solution during evaporation, which comprises adding to the condenser water used in condensing the steam from the evaporator alkali-metal phosphate having a ratio of NazO to P205 between 0.9:1 and 1.7:1 between about 42 P. P. M; and 10P. P. M. based on the weight of the condenser water, and utilizing the thus treated condenser water in extracting sugar to ymake sugar solution which is to be evaporated.

4. In the treatment of sugar solutions contain- 6. In the treatment of sugar solutions containing alkaline earth metal salts, the process of inhibiting the formation of scale on surfaces in contact with said solution during evaporation, which comprises ladding to the sugar solution during evaporation thereof,` molecularly dehydrated alkali-metal phosphate in lamount between about 2 P. P. M. and 10 P. P. M. based on the weight of the sugar solution entering the rst effect evaporator.

7. In the treatment of sugar solutions contain,- ing alkaline earthmetal salts, the process of in.- hibiting the formation of scale on surfaces in `contact with said solution during evaporation,

whichl comprises adding to the sugar solution during evaporation thereof, glassy molecularly dehydrated alkali-metal phosphate having a ratio of Na-l0 to P205 between 0.9:1 and 1.7:1,.in

amount between about 2 P. P. M. and 1o P. P. M.4

based,on the weight ofthe sugar solution entering the first eifect'evaporator.

R. ALLEN. 

